Electronic Supplementary Material for CrystEngComm This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_name_full CrystEngComm _journal_coden_cambridge 1350 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Jhy-Der Chen' _publ_contact_author_email JDCHEN@CYCU.EDU.TW loop_ _publ_author_name 'Jhy-Der Chen' 'Zhi-Kai Chan' 'Chih-Yuan Lin' 'Ju-Chun Wang' ; Chia-Jun Wu ; 'Chun-Wei Yeh' data_1 _database_code_depnum_ccdc_archive 'CCDC 616573' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H19 Ag4 I4 N17 O12' _chemical_formula_weight 1604.58 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M P4(2)/nmc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' '-y+1/2, x, z+1/2' 'y, -x+1/2, z+1/2' '-x, y+1/2, -z' 'x+1/2, -y, -z' 'y+1/2, x+1/2, -z+1/2' '-y, -x, -z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z' 'y-1/2, -x, -z-1/2' '-y, x-1/2, -z-1/2' 'x, -y-1/2, z' '-x-1/2, y, z' '-y-1/2, -x-1/2, z-1/2' 'y, x, z-1/2' _cell_length_a 16.9297(12) _cell_length_b 16.9297(12) _cell_length_c 6.7285(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1928.5(3) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 50 _cell_measurement_theta_min 5.10 _cell_measurement_theta_max 12.52 _exptl_crystal_description column _exptl_crystal_colour colorless _exptl_crystal_size_max 0.75 _exptl_crystal_size_mid 0.55 _exptl_crystal_size_min 0.40 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.763 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1484 _exptl_absorpt_coefficient_mu 5.279 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8331 _exptl_absorpt_correction_T_max 0.9757 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 300 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 3.25 _diffrn_reflns_number 1758 _diffrn_reflns_av_R_equivalents 0.0184 _diffrn_reflns_av_sigmaI/netI 0.0244 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 2.41 _diffrn_reflns_theta_max 24.99 _reflns_number_total 907 _reflns_number_gt 749 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0201P)^2^+1.0531P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00123(10) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 907 _refine_ls_number_parameters 89 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0320 _refine_ls_R_factor_gt 0.0222 _refine_ls_wR_factor_ref 0.0492 _refine_ls_wR_factor_gt 0.0466 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_restrained_S_all 1.038 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag Ag 0.062730(19) 0.562730(19) 0.7500 0.04481(16) Uani 1 2 d S . . I1A I 0.2500 0.35414(14) 0.2097(3) 0.0629(6) Uani 0.50 2 d SP . . I1B I 0.2500 0.37384(13) 0.1485(3) 0.0491(4) Uani 0.50 2 d SP . . N1 N 0.17913(17) 0.50420(18) 0.6791(5) 0.0409(7) Uani 1 1 d . . . N2 N 0.2500 0.5669(4) 0.9257(10) 0.075(2) Uani 1 2 d S . . C1 C 0.2500 0.4350(3) 0.4302(8) 0.0378(12) Uani 1 2 d S . . C2 C 0.1806(2) 0.4593(2) 0.5170(6) 0.0387(8) Uani 1 1 d . . . C3 C 0.2500 0.5246(3) 0.7591(8) 0.0437(12) Uani 1 2 d S . . N3 N -0.06893(19) 0.43107(19) 0.7500 0.0455(11) Uani 1 2 d S . . O1 O -0.01316(18) 0.4276(2) 0.6309(4) 0.0690(9) Uani 1 1 d . . . O2 O -0.1194(2) 0.3806(2) 0.7500 0.102(2) Uani 1 2 d S . . H2N H 0.290(3) 0.571(3) 0.984(7) 0.088(19) Uiso 1 1 d . . . H2 H 0.129(2) 0.446(2) 0.470(5) 0.045(11) Uiso 1 1 d . . . C6 C -0.2500 0.2500 0.7500 0.196(14) Uiso 1 8 d SD . . C5 C -0.279(2) 0.2500 0.953(2) 0.14(2) Uiso 0.25 2 d SPD . . N4 N -0.304(3) 0.2500 1.112(3) 0.31(4) Uiso 0.25 2 d SPD . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag 0.04413(18) 0.04413(18) 0.0462(3) -0.00381(13) 0.00381(13) 0.01223(18) I1A 0.0447(6) 0.0778(15) 0.0663(14) -0.0416(10) 0.000 0.000 I1B 0.0530(6) 0.0429(8) 0.0513(11) -0.0139(6) 0.000 0.000 N1 0.0325(15) 0.0465(17) 0.0435(17) -0.0051(15) -0.0006(14) 0.0042(14) N2 0.034(3) 0.130(6) 0.061(4) -0.044(4) 0.000 0.000 C1 0.040(3) 0.030(3) 0.043(3) -0.007(2) 0.000 0.000 C2 0.034(2) 0.0350(19) 0.047(2) -0.0008(17) -0.0014(17) 0.0017(16) C3 0.043(3) 0.048(3) 0.040(3) -0.006(3) 0.000 0.000 N3 0.0440(15) 0.0440(15) 0.048(2) -0.0001(18) 0.0001(18) 0.000(2) O1 0.0534(18) 0.106(3) 0.0471(18) 0.0089(17) 0.0109(15) 0.0115(17) O2 0.071(2) 0.071(2) 0.166(6) -0.017(3) 0.017(3) -0.028(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag N1 2.257(3) 7_456 ? Ag N1 2.257(3) . ? I1A I1B 0.530(3) . ? I1A C1 2.019(6) . ? I1B C1 2.160(6) . ? N1 C2 1.330(5) . ? N1 C3 1.360(4) . ? N2 C3 1.330(8) . ? N2 H2N 0.78(5) . ? C1 C2 1.376(4) 14_655 ? C1 C2 1.376(4) . ? C2 H2 0.95(4) . ? C3 N1 1.360(4) 14_655 ? N3 O2 1.208(7) . ? N3 O1 1.240(4) 7_456 ? N3 O1 1.240(4) . ? C6 C5 1.4500(18) 12_567 ? C6 C5 1.4500(18) 11_557 ? C6 C5 1.4500(18) 2_455 ? C6 C5 1.4500(19) . ? C5 C5 0.97(8) 2_455 ? C5 N4 1.1502(19) . ? C5 N4 1.76(5) 2_455 ? N4 C5 1.76(5) 2_455 ? N4 N4 1.81(11) 2_455 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ag N1 144.25(15) 7_456 . ? I1B I1A C1 98.3(6) . . ? I1A I1B C1 67.6(5) . . ? C2 N1 C3 117.0(3) . . ? C2 N1 Ag 116.1(2) . . ? C3 N1 Ag 125.1(3) . . ? C3 N2 H2N 118(4) . . ? C2 C1 C2 117.4(5) 14_655 . ? C2 C1 I1A 121.0(2) 14_655 . ? C2 C1 I1A 121.0(2) . . ? C2 C1 I1B 121.1(3) 14_655 . ? C2 C1 I1B 121.1(3) . . ? I1A C1 I1B 14.05(9) . . ? N1 C2 C1 122.4(4) . . ? N1 C2 H2 113(2) . . ? C1 C2 H2 125(2) . . ? N2 C3 N1 118.1(2) . . ? N2 C3 N1 118.1(2) . 14_655 ? N1 C3 N1 123.9(5) . 14_655 ? O2 N3 O1 120.4(3) . 7_456 ? O2 N3 O1 120.4(3) . . ? O1 N3 O1 119.3(5) 7_456 . ? C5 C6 C5 39(3) 12_567 11_557 ? C5 C6 C5 153(2) 12_567 2_455 ? C5 C6 C5 153(2) 11_557 2_455 ? C5 C6 C5 153(2) 12_567 . ? C5 C6 C5 153(2) 11_557 . ? C5 C6 C5 39(3) 2_455 . ? C5 C5 N4 112(4) 2_455 . ? C5 C5 C6 70.5(17) 2_455 . ? N4 C5 C6 178(5) . . ? C5 C5 N4 37.5(16) 2_455 2_455 ? N4 C5 N4 74(5) . 2_455 ? C6 C5 N4 108(2) . 2_455 ? C5 N4 C5 31(3) . 2_455 ? C5 N4 N4 68(4) . 2_455 ? C5 N4 N4 37.5(16) 2_455 2_455 ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.570 _refine_diff_density_min -0.544 _refine_diff_density_rms 0.074 #===END data_2 _database_code_depnum_ccdc_archive 'CCDC 616574' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C4 H4 Ag F6 I N3 P' _chemical_formula_weight 473.84 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M I4(1)/a loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-y+3/4, x+1/4, z+1/4' 'y+3/4, -x+3/4, z+3/4' 'x+1/2, y+1/2, z+1/2' '-x+1, -y+1/2, z+1' '-y+5/4, x+3/4, z+3/4' 'y+5/4, -x+5/4, z+5/4' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'y-3/4, -x-1/4, -z-1/4' '-y-3/4, x-3/4, -z-3/4' '-x+1/2, -y+1/2, -z+1/2' 'x, y+1/2, -z' 'y-1/4, -x+1/4, -z+1/4' '-y-1/4, x-1/4, -z-1/4' _cell_length_a 18.711(3) _cell_length_b 18.711(3) _cell_length_c 22.584(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7906.3(19) _cell_formula_units_Z 16 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 32 _cell_measurement_theta_min 4.85 _cell_measurement_theta_max 12.47 _exptl_crystal_description block _exptl_crystal_colour pale_yellow _exptl_crystal_size_max 0.65 _exptl_crystal_size_mid 0.60 _exptl_crystal_size_min 0.45 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.592 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3488 _exptl_absorpt_coefficient_mu 2.695 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7857 _exptl_absorpt_correction_T_max 0.9560 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 297 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 7.05 _diffrn_reflns_number 3456 _diffrn_reflns_av_R_equivalents 0.0342 _diffrn_reflns_av_sigmaI/netI 0.0944 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.18 _diffrn_reflns_theta_max 24.50 _reflns_number_total 3240 _reflns_number_gt 1167 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0142P)^2^+15.2270P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3240 _refine_ls_number_parameters 145 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0995 _refine_ls_R_factor_gt 0.0481 _refine_ls_wR_factor_ref 0.1133 _refine_ls_wR_factor_gt 0.1030 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_restrained_S_all 1.034 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 -0.015 -0.003 -0.003 3787.7 2589.5 _platon_squeeze_details ; A. L. Spek, J Appl. Cryst., 2003, 36, 7-13. ; loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group I I 0.55839(4) 0.65434(4) 0.01630(3) 0.1115(3) Uani 1 1 d . . . Ag Ag 0.34322(5) 0.47084(5) -0.11159(4) 0.1245(4) Uani 1 1 d . . . N1 N 0.3709(5) 0.5352(5) -0.0346(3) 0.090(3) Uani 1 1 d . . . N2 N 0.2662(5) 0.5030(6) 0.0147(5) 0.167(6) Uani 1 1 d . . . H2B H 0.2388 0.5072 0.0452 0.200 Uiso 1 1 calc R . . H2C H 0.2530 0.4771 -0.0147 0.200 Uiso 1 1 calc R . . N3 N 0.3466(5) 0.5764(5) 0.0603(4) 0.095(3) Uani 1 1 d . . . C1 C 0.3259(7) 0.5352(7) 0.0133(5) 0.104(4) Uani 1 1 d . . . C2 C 0.4335(6) 0.5702(6) -0.0332(4) 0.094(4) Uani 1 1 d . . . H2A H 0.4621 0.5686 -0.0668 0.113 Uiso 1 1 calc R . . C3 C 0.4578(5) 0.6080(5) 0.0142(4) 0.086(3) Uani 1 1 d . . . C4 C 0.4109(8) 0.6106(6) 0.0612(4) 0.103(4) Uani 1 1 d . . . H4A H 0.4235 0.6367 0.0947 0.124 Uiso 1 1 calc R . . P P 0.5178(3) 0.5137(3) -0.2077(2) 0.1553(17) Uani 1 1 d . . . F1 F 0.6001(5) 0.4823(5) -0.2076(4) 0.203(4) Uani 1 1 d . . . F2 F 0.5386(6) 0.5718(7) -0.1606(5) 0.288(6) Uani 1 1 d . . . F3 F 0.4962(5) 0.4575(6) -0.1578(4) 0.232(5) Uani 1 1 d . . . F4 F 0.5384(7) 0.5716(6) -0.2537(5) 0.293(7) Uani 1 1 d . . . F5 F 0.4943(9) 0.4563(7) -0.2538(5) 0.353(9) Uani 1 1 d . . . F6 F 0.4333(7) 0.5412(6) -0.2074(5) 0.276(6) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 I 0.1110(6) 0.1364(7) 0.0872(5) -0.0118(5) -0.0073(5) -0.0038(5) Ag 0.1425(9) 0.1611(9) 0.0699(5) -0.0433(6) -0.0099(6) -0.0069(7) N1 0.111(7) 0.101(7) 0.058(5) -0.024(5) 0.003(5) 0.002(6) N2 0.111(9) 0.231(14) 0.158(11) -0.052(9) 0.056(8) -0.066(9) N3 0.104(8) 0.107(8) 0.073(6) -0.013(6) 0.020(6) 0.016(6) C1 0.149(12) 0.120(10) 0.042(6) -0.025(7) 0.024(8) 0.014(9) C2 0.103(9) 0.132(11) 0.048(6) -0.041(6) -0.001(6) 0.027(8) C3 0.097(8) 0.100(8) 0.060(6) -0.012(6) -0.002(6) 0.017(7) C4 0.160(13) 0.115(10) 0.035(6) -0.005(6) -0.008(8) 0.043(9) P 0.204(6) 0.158(4) 0.104(3) 0.003(3) 0.028(3) 0.048(4) F1 0.169(8) 0.234(10) 0.207(9) -0.008(8) 0.037(7) 0.054(7) F2 0.285(13) 0.318(14) 0.259(12) -0.154(12) 0.085(10) -0.063(11) F3 0.200(9) 0.294(13) 0.202(9) 0.075(10) 0.028(7) 0.048(8) F4 0.466(19) 0.221(11) 0.193(9) 0.091(9) 0.151(11) 0.029(11) F5 0.58(3) 0.332(16) 0.147(8) -0.106(11) -0.052(12) 0.132(16) F6 0.305(14) 0.189(10) 0.334(14) 0.053(10) -0.004(12) 0.084(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag I C3 2.073(10) . ? Ag N1 2.178(8) . ? Ag N3 2.192(8) 4_454 ? N1 C2 1.342(11) . ? N1 C1 1.371(12) . ? N2 C1 1.269(13) . ? N3 C4 1.362(12) . ? N3 C1 1.368(13) . ? N3 Ag 2.192(8) 3 ? C2 C3 1.361(12) . ? C3 C4 1.379(12) . ? P F4 1.550(10) . ? P F5 1.557(12) . ? P F2 1.572(10) . ? P F3 1.594(10) . ? P F1 1.648(9) . ? P F6 1.662(12) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ag N3 174.4(4) . 4_454 ? C2 N1 C1 121.2(9) . . ? C2 N1 Ag 119.7(7) . . ? C1 N1 Ag 118.9(8) . . ? C4 N3 C1 121.9(10) . . ? C4 N3 Ag 115.4(8) . 3 ? C1 N3 Ag 122.8(9) . 3 ? N2 C1 N3 119.8(11) . . ? N2 C1 N1 124.1(12) . . ? N3 C1 N1 115.9(12) . . ? N1 C2 C3 124.3(10) . . ? C2 C3 C4 114.3(10) . . ? C2 C3 I 122.6(9) . . ? C4 C3 I 123.1(9) . . ? N3 C4 C3 122.2(10) . . ? F4 P F5 96.0(7) . . ? F4 P F2 84.8(7) . . ? F5 P F2 178.0(8) . . ? F4 P F3 176.8(7) . . ? F5 P F3 87.0(7) . . ? F2 P F3 92.2(6) . . ? F4 P F1 91.0(6) . . ? F5 P F1 91.1(7) . . ? F2 P F1 90.8(7) . . ? F3 P F1 90.0(5) . . ? F4 P F6 91.4(7) . . ? F5 P F6 87.0(8) . . ? F2 P F6 91.1(6) . . ? F3 P F6 87.7(6) . . ? F1 P F6 177.1(7) . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 24.50 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 0.557 _refine_diff_density_min -0.381 _refine_diff_density_rms 0.088 #===END data_3 _database_code_depnum_ccdc_archive 'CCDC 616575' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C4 H4 Ag Cl I N3 O4' _chemical_formula_weight 428.32 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pnna loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z' '-x+1/2, y+1/2, -z+1/2' 'x, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z' 'x-1/2, -y-1/2, z-1/2' '-x, y-1/2, z-1/2' _cell_length_a 19.1267(17) _cell_length_b 11.4655(9) _cell_length_c 9.0154(13) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1977.1(4) _cell_formula_units_Z 8 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 34 _cell_measurement_theta_min 3.55 _cell_measurement_theta_max 18.38 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.878 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1584 _exptl_absorpt_coefficient_mu 5.424 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.5224 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 100 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 2320 _diffrn_reflns_av_R_equivalents 0.0368 _diffrn_reflns_av_sigmaI/netI 0.0408 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 1 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 1 _diffrn_reflns_limit_l_min -1 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.13 _diffrn_reflns_theta_max 25.00 _reflns_number_total 1741 _reflns_number_gt 1227 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0185P)^2^+28.8658P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00025(5) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 1741 _refine_ls_number_parameters 130 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0791 _refine_ls_R_factor_gt 0.0501 _refine_ls_wR_factor_ref 0.1091 _refine_ls_wR_factor_gt 0.0983 _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_restrained_S_all 1.052 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group I I 0.43992(4) -0.06851(7) -0.27658(10) 0.0610(3) Uani 1 1 d . . . Ag1 Ag 0.60047(7) -0.2500 0.2500 0.0735(5) Uani 1 2 d S . . Ag2 Ag 0.7500 0.0000 -0.26202(15) 0.0575(4) Uani 1 2 d S . . N1 N 0.6016(4) -0.1924(8) 0.0192(9) 0.043(2) Uani 1 1 d . . . N2 N 0.7207(4) -0.2019(8) -0.0073(10) 0.053(2) Uani 1 1 d . . . H2A H 0.7245 -0.2454 0.0768 0.063 Uiso 1 1 d R . . H2B H 0.7527 -0.2115 -0.0831 0.063 Uiso 1 1 d R . . N3 N 0.6597(4) -0.1059(7) -0.1878(9) 0.0376(19) Uani 1 1 d . . . C1 C 0.6599(5) -0.1674(8) -0.0608(10) 0.035(2) Uani 1 1 d . . . C2 C 0.5982(5) -0.0796(9) -0.2464(12) 0.043(2) Uani 1 1 d . . . H2C H 0.5970 -0.0402 -0.3365 0.052 Uiso 1 1 calc R . . C3 C 0.5358(5) -0.1084(8) -0.1789(10) 0.036(2) Uani 1 1 d . . . C4 C 0.5399(5) -0.1624(9) -0.0425(12) 0.048(3) Uani 1 1 d . . . H4A H 0.4988 -0.1787 0.0086 0.058 Uiso 1 1 calc R . . Cl1 Cl 0.7500 0.0000 -0.6256(4) 0.0562(10) Uani 1 2 d S . . Cl2 Cl 0.60958(19) 0.2500 0.7500 0.0544(10) Uani 1 2 d S . . O1 O 0.8085(5) -0.0083(12) -0.5314(11) 0.111(4) Uani 1 1 d . . . O2 O 0.7439(9) -0.0969(10) -0.7132(11) 0.132(5) Uani 1 1 d . . . O3 O 0.5638(11) 0.3113(13) 0.821(2) 0.267(14) Uani 1 1 d . . . O4 O 0.6450(7) 0.1701(10) 0.826(3) 0.224(11) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 I 0.0409(4) 0.0682(5) 0.0739(6) 0.0020(5) -0.0175(4) 0.0025(4) Ag1 0.0587(8) 0.1240(13) 0.0379(7) 0.0238(8) 0.000 0.000 Ag2 0.0416(6) 0.0701(8) 0.0607(8) 0.000 0.000 -0.0181(6) N1 0.042(5) 0.053(5) 0.034(4) 0.005(4) 0.004(4) 0.005(4) N2 0.043(5) 0.078(6) 0.037(5) 0.004(5) 0.004(4) 0.018(5) N3 0.038(4) 0.039(4) 0.036(4) 0.004(4) 0.001(4) 0.001(4) C1 0.033(5) 0.044(6) 0.029(5) -0.009(5) 0.001(4) -0.003(5) C2 0.045(5) 0.042(5) 0.043(5) 0.003(6) -0.001(5) 0.003(5) C3 0.030(5) 0.044(6) 0.034(5) -0.004(5) -0.004(4) 0.000(4) C4 0.035(5) 0.060(7) 0.048(6) -0.005(6) 0.004(5) 0.002(5) Cl1 0.049(2) 0.075(3) 0.045(2) 0.000 0.000 -0.004(2) Cl2 0.0386(19) 0.062(2) 0.062(2) -0.006(2) 0.000 0.000 O1 0.051(5) 0.207(12) 0.076(6) -0.038(8) -0.015(5) 0.023(7) O2 0.223(14) 0.104(8) 0.069(7) -0.034(6) -0.011(9) -0.035(9) O3 0.39(3) 0.128(12) 0.28(2) 0.095(14) 0.27(2) 0.101(15) O4 0.159(12) 0.082(8) 0.43(3) 0.004(13) -0.199(17) 0.024(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag I C3 2.085(9) . ? Ag1 N1 2.184(8) 4_545 ? Ag1 N1 2.184(8) . ? Ag2 N3 2.215(8) 2_655 ? Ag2 N3 2.215(8) . ? N1 C4 1.348(12) . ? N1 C1 1.358(12) . ? N2 C1 1.320(12) . ? N2 H2A 0.9105 . ? N2 H2B 0.9240 . ? N3 C2 1.325(12) . ? N3 C1 1.345(12) . ? C2 C3 1.380(13) . ? C2 H2C 0.9300 . ? C3 C4 1.379(14) . ? C4 H4A 0.9300 . ? Cl1 O2 1.368(10) . ? Cl1 O2 1.368(10) 2_655 ? Cl1 O1 1.408(9) 2_655 ? Cl1 O1 1.408(9) . ? Cl2 O3 1.294(14) 4_556 ? Cl2 O3 1.294(14) . ? Cl2 O4 1.329(13) . ? Cl2 O4 1.329(13) 4_556 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ag1 N1 178.9(4) 4_545 . ? N3 Ag2 N3 144.8(4) 2_655 . ? C4 N1 C1 116.5(8) . . ? C4 N1 Ag1 117.5(7) . . ? C1 N1 Ag1 125.3(6) . . ? C1 N2 H2A 122.6 . . ? C1 N2 H2B 110.5 . . ? H2A N2 H2B 119.8 . . ? C2 N3 C1 117.5(9) . . ? C2 N3 Ag2 116.6(6) . . ? C1 N3 Ag2 122.9(6) . . ? N2 C1 N3 118.0(9) . . ? N2 C1 N1 117.8(9) . . ? N3 C1 N1 124.1(9) . . ? N3 C2 C3 122.6(9) . . ? N3 C2 H2C 118.7 . . ? C3 C2 H2C 118.7 . . ? C2 C3 C4 116.8(9) . . ? C2 C3 I 121.5(7) . . ? C4 C3 I 121.7(7) . . ? N1 C4 C3 122.1(9) . . ? N1 C4 H4A 118.9 . . ? C3 C4 H4A 118.9 . . ? O2 Cl1 O2 109.4(10) . 2_655 ? O2 Cl1 O1 109.6(8) . 2_655 ? O2 Cl1 O1 111.2(8) 2_655 2_655 ? O2 Cl1 O1 111.2(8) . . ? O2 Cl1 O1 109.6(8) 2_655 . ? O1 Cl1 O1 105.8(8) 2_655 . ? O3 Cl2 O3 95(2) 4_556 . ? O3 Cl2 O4 103.0(8) 4_556 . ? O3 Cl2 O4 117.7(13) . . ? O3 Cl2 O4 117.7(13) 4_556 4_556 ? O3 Cl2 O4 103.0(8) . 4_556 ? O4 Cl2 O4 118.7(16) . 4_556 ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.933 _refine_diff_density_min -0.979 _refine_diff_density_rms 0.162 #===END